CN108383678B - Durene separation and purification method based on bubble fractional crystallization and distillation - Google Patents
Durene separation and purification method based on bubble fractional crystallization and distillation Download PDFInfo
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Abstract
The invention provides a durene separation and purification method based on bubble fractional crystallization and distillation, which is characterized by comprising the following steps: the method comprises the following steps: adding a durene-containing material into a crystallizer, introducing small nitrogen bubbles from bottom to top, cooling to-10 to-15 ℃, then cooling to-25 to-30 ℃, carrying out crystallization treatment, introducing the small nitrogen bubbles from top to bottom, and filtering crystals precipitated by crystallization through an inclined porous sieve to obtain a durene crude product; heating and melting the durene crude product, introducing small nitrogen bubbles from bottom to top, heating to 190 ℃, continuing heating to 196 ℃ and 198 ℃, carrying out heat preservation treatment, and condensing and recovering steam to obtain the separated and purified durene. The invention accelerates the crystallization and evaporation efficiency of durene by utilizing the bubble technology, obviously improves the separation and purification efficiency of durene by utilizing the accurate temperature control technology on the basis of reducing energy consumption, is simple and efficient, has strong controllability and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of durene separation, and particularly relates to a durene separation and purification method based on bubble fractional crystallization and distillation.
Background
Durene, namely 1,2,4, 5-tetramethylbenzene, has symmetrical dipole pairs, the boiling point of which is 196.8 ℃, the melting point of which is 79.2 ℃, is higher than the isomers of the durene and the durene, camphor odor, white crystals, is soluble in organic solvents such as ether, ethanol and the like, is insoluble in water and can be sublimated, and derived polymers of the durene have stepwise alternate single bonds and double bonds and have good high-temperature resistance, so the market demand is increasing.
Durene can be obtained by separation or isomerization and other synthetic reactions from C10 aromatic hydrocarbon at present, wherein the traditional separation and purification technology is to firstly rectify and cut fractions with different boiling points from C10 aromatic hydrocarbon, then separate out a crude durene product by freezing crystallization, then obtain the durene product by squeezing separation, and simultaneously recover mother liquor obtained by centrifugation and squeezing to be used as raw materials of the isomerization reaction. The method for extracting durene from C10 heavy aromatics disclosed in Chinese patent CN 1028358C comprises the steps of feeding durene rich liquid obtained by rectification separation from C10 heavy aromatics into a distributed crystallization tower, separating out crystals in the crystallization tower, purifying and separating the crystals, repeatedly melting and crystallizing durene by composite alternating temperature rise, and improving the concentration and purity of durene. The process method for producing durene by reforming the decaaromatic hydrocarbon disclosed in the Chinese patent CN101279886B comprises the steps of passing the reformed decaaromatic hydrocarbon through at least a first rectifying tower (the tower top temperature is 125-. The method combines continuous rectification technology with refrigeration temperature increase, reduces the requirements of the process on equipment, reduces production cost and energy consumption, and has the product yield of 80% and the product purity of 99%.
According to the prior art, durene with different yields and purities can be obtained by performing different crystallization and purification on the rectified durene enrichment liquid, but the preparation method has the advantages of complex process route, high energy consumption, low controllability, low working efficiency, poor production environment and great promotion space for the purity and yield of durene.
Disclosure of Invention
The invention aims to solve the technical problem of providing a durene separation and purification method based on bubble fractional crystallization and distillation, which accelerates the crystallization and evaporation efficiency of durene by utilizing a bubble technology, obviously improves the durene separation and purification efficiency on the basis of reducing energy consumption by using an accurate temperature control technology, is simple and efficient, has strong controllability and is suitable for industrial production.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a durene separation and purification method based on bubble fractional crystallization and distillation is characterized in that: the method comprises the following steps:
(1) adding a material containing durene into a crystallizer, introducing small nitrogen bubbles from bottom to top, cooling to-10 to-15 ℃, then cooling to-25 to-30 ℃ at the speed of 0.5-1 ℃/min, carrying out crystallization treatment, introducing the small nitrogen bubbles from top to bottom, filtering crystals settled by crystallization through an inclined porous sieve at the temperature of 56-60 ℃, and treating for 5-50min to obtain a durene crude product;
(2) heating and melting the durene crude product prepared in the step (1), introducing small nitrogen bubbles from bottom to top, heating to 190 ℃ at the speed of 5-10 ℃/min, continuing heating to 196 ℃ at the speed of 0.1-0.5 ℃/min, keeping the temperature at 198 ℃, condensing and recovering steam, and obtaining the separated and purified durene.
Preferably, in the step (1), the durene content in the durene-containing material is not less than 45%.
Preferably, in the step (1), the gas velocity of the small nitrogen bubbles introduced from bottom to top is 40-60L/h.
Preferably, in the step (1), the crystallization is performed for 50 to 90 min.
Preferably, in the step (1), the gas velocity of the small nitrogen bubbles introduced from top to bottom is 30-50L/h.
Preferably, in the step (1), the nano-scale metal particles are attached to the porous sieve.
Preferably, in the step (1), the inclined angle of the inclined porous sieve is 45-50 degrees, and the aperture of the porous sieve is 0.5-5 mm.
Preferably, in the step (2), the temperature for heating and melting is 130-135 ℃.
Preferably, in the step (2), the gas velocity of the small nitrogen bubbles introduced from bottom to top is 15-45L/h.
Preferably, in the step (2), the purity of the durene separated and purified is 99.7-99.8%, and the yield is 95-98%.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention relates to a durene separation and purification method based on bubble fractional crystallization and distillation, which utilizes a bubble technology to accelerate the crystallization and evaporation efficiency of durene, in the process of temperature reduction and temperature rise, a thin liquid film is arranged around small bubbles to be reduced in a turbulent state by introducing small bubbles of nitrogen, so that the transfer resistance of heat is greatly reduced, and part of small bubbles are converged and form large bubbles in the process of rising, thereby generating vortex, further promoting the mass transfer of heat in durene enrichment liquid, improving the efficiency of cooling and heating, achieving the purposes of low energy consumption and high efficiency, changing the direction of introducing small bubbles of nitrogen in the process of filtering, promoting the settling velocity of small crystals formed in a system, facilitating the tiny crystals suspended in the system to pass through a porous sieve, and reducing the existence of adhering or coating impurities on the surface and inside of the crystals, the separation efficiency and the purity of the product are improved. In addition, the invention also controls the temperature of the porous sieve in the crystal sedimentation and filtration process, so that the crystal is subjected to sweating treatment in the filtration process, and the sweating effect is obvious because the crystal particles passing through the filtration are tiny, and the porous sieve is inclined at an angle, so that the particle filtration path is increased, the sweating treatment time is prolonged, the sweating treatment is sufficient, the removal rate of the coating liquid in the crystal is improved, and the separation efficiency and the purity of the product are further improved.
(2) According to the method for separating and purifying durene based on bubble fractional crystallization and distillation, the temperature is accurately controlled according to the boiling point of durene of 196.84 ℃, the melting point of 79.23 ℃, the boiling point of pseudocumene of 169.38 ℃, the melting point of-43.77 ℃, the boiling point of pseudocumene of 198.04 ℃, the melting point of-23.67 ℃, the boiling point of pentamethylene of 232 ℃ and the melting point of 54.2 ℃, and the existence of impurities adhered or coated on the surface and the interior of a crystal is reduced by adopting the step-by-step heating and cooling technology, so that the production energy consumption is reduced, the separation efficiency of the product is high, and the purity is high.
(3) The preparation method disclosed by the invention is simple, strong in controllability, simple and efficient, and suitable for industrial production, and the separation and purification efficiency of durene is remarkably improved on the basis of reducing energy consumption.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1:
(1) adding a material containing 50% of durene into a crystallizer, introducing small nitrogen bubbles with the flow rate of 40L/h from bottom to top, firstly cooling to-10 ℃, then cooling to-25 ℃ at the speed of 0.5 ℃/min, carrying out crystallization treatment for 50min, introducing small nitrogen bubbles with the flow rate of 30L/h from top to bottom, and filtering crystals deposited by crystallization for 5min through a porous sieve which is inclined at 45 degrees at 56 ℃ and is attached with nano-scale metal particles, wherein the pore diameter of the porous sieve is 0.5-1mm, thus obtaining a durene crude product.
(2) Heating and melting the durene crude product at 130 ℃, introducing small nitrogen bubbles with the flow rate of 15L/h from bottom to top, heating to 190 ℃ at the speed of 5 ℃/min, then continuously heating to 196 ℃ at the speed of 0.1 ℃/min for heat preservation treatment, condensing and recovering steam, and obtaining the separated and purified durene.
Example 2:
(1) adding a material containing 55% of durene into a crystallizer, introducing small nitrogen bubbles with the flow rate of 60L/h from bottom to top, firstly cooling to-15 ℃, then cooling to-30 ℃ at the speed of 1 ℃/min, carrying out crystallization treatment for 90min, introducing small nitrogen bubbles with the flow rate of 50L/h from top to bottom, filtering crystals deposited by crystallization for 50min through a porous sieve which is inclined at the temperature of 60 ℃ by 50 degrees and is attached with nano-scale metal particles, wherein the pore diameter of the porous sieve is 3-5mm, and obtaining a durene crude product.
(2) Heating and melting the durene crude product at 135 ℃, introducing small nitrogen bubbles with the flow rate of 45L/h from bottom to top, heating to 190 ℃ at the speed of 10 ℃/min, then continuously heating to 198 ℃ at the speed of 0.5 ℃/min, carrying out heat preservation treatment, condensing and recovering steam, and obtaining the separated and purified durene.
Example 3:
(1) adding a material containing 60% of durene into a crystallizer, introducing small nitrogen bubbles with the flow rate of 55L/h from bottom to top, firstly cooling to-13 ℃, then cooling to-24 ℃ at the speed of 0.7 ℃/min, carrying out crystallization treatment for 60min, introducing small nitrogen bubbles with the flow rate of 35L/h from top to bottom, and filtering crystals deposited by crystallization for 30min through a porous sieve which is inclined at the temperature of 57 ℃ by 48 degrees and is attached with nano-scale metal particles, wherein the pore diameter of the porous sieve is 1-3mm, thus obtaining a durene crude product.
(2) Heating and melting the durene crude product at 132 ℃, introducing small nitrogen bubbles with the flow rate of 20L/h from bottom to top, heating to 190 ℃ at the speed of 7 ℃/min, then continuously heating to 197 ℃ at the speed of 0.2 ℃/min for heat preservation treatment, condensing and recovering steam, and obtaining the separated and purified durene.
Example 4:
(1) adding a material containing 55% of durene into a crystallizer, introducing small nitrogen bubbles with the flow rate of 45L/h from bottom to top, firstly cooling to-13 ℃, then cooling to-26 ℃ at the speed of 0.8 ℃/min, carrying out crystallization treatment for 75min, introducing small nitrogen bubbles with the flow rate of 35L/h from top to bottom, and filtering crystals deposited by crystallization for 30min through a porous sieve which is inclined at 58 ℃ by 49 degrees and is attached with nano-scale metal particles, wherein the pore diameter of the porous sieve is 0.5-2mm, thus obtaining a durene crude product.
(2) Heating and melting the durene crude product at 134 ℃, introducing small nitrogen bubbles with the flow rate of 30L/h from bottom to top, heating to 190 ℃ at the speed of 6 ℃/min, then continuously heating to 197.5 ℃ at the speed of 0.4 ℃/min, carrying out heat preservation treatment, condensing and recovering steam, and obtaining the separated and purified durene.
Example 5:
(1) adding a material containing 50% of durene into a crystallizer, introducing small nitrogen bubbles with the flow rate of 45L/h from bottom to top, firstly cooling to-11 ℃, then cooling to-30 ℃ at the speed of 0.8 ℃/min, carrying out crystallization treatment for 80min, introducing small nitrogen bubbles with the flow rate of 35L/h from top to bottom, and filtering crystals settled by crystallization for 40min through a porous sieve which is inclined at 49 degrees at 59 ℃ and is attached with nano-scale metal particles, wherein the pore diameter of the porous sieve is 3-5mm, thus obtaining a durene crude product.
(2) Heating and melting the durene crude product at 133 ℃, introducing small nitrogen bubbles with the flow rate of 25L/h from bottom to top, heating to 190 ℃ at the speed of 6 ℃/min, then continuously heating to 197 ℃ at the speed of 0.4 ℃/min for heat preservation treatment, condensing and recovering steam, and obtaining the separated and purified durene.
Example 6:
(1) adding a material containing 50% of durene into a crystallizer, introducing small nitrogen bubbles with the flow rate of 40L/h from bottom to top, firstly cooling to-12 ℃, then cooling to-28 ℃ at the speed of 0.5 ℃/min, carrying out crystallization treatment for 50min, introducing small nitrogen bubbles with the flow rate of 50L/h from top to bottom, and filtering crystals deposited by crystallization for 5min through a porous sieve which is inclined at the temperature of 56 ℃ by 50 degrees and is attached with nano-scale metal particles, wherein the pore diameter of the porous sieve is 4-5mm, thus obtaining a durene crude product.
(2) Heating and melting the durene crude product at 130 ℃, introducing small nitrogen bubbles with the flow rate of 45L/h from bottom to top, heating to 190 ℃ at the speed of 5 ℃/min, then continuously heating to 196 ℃ at the speed of 0.5 ℃/min for heat preservation treatment, condensing and recovering steam, and obtaining the separated and purified durene.
Example 7:
(1) adding a material containing 60% of durene into a crystallizer, introducing small nitrogen bubbles with the flow rate of 60L/h from bottom to top, firstly cooling to-15 ℃, then cooling to-30 ℃ at the speed of 1 ℃/min, carrying out crystallization treatment for 90min, introducing small nitrogen bubbles with the flow rate of 30L/h from top to bottom, filtering crystals deposited by crystallization for 50min through a porous sieve which is inclined at 45 degrees at 60 ℃ and is attached with nano-scale metal particles, wherein the pore diameter of the porous sieve is 0.5-1.5mm, and obtaining a durene crude product.
(2) Heating and melting the durene crude product at 135 ℃, introducing small nitrogen bubbles with the flow rate of 15L/h from bottom to top, heating to 190 ℃ at the speed of 10 ℃/min, then continuously heating to 198 ℃ at the speed of 0.1 ℃/min, carrying out heat preservation treatment, condensing and recovering steam, and obtaining the separated and purified durene.
Comparative example 1:
(1) adding a material containing 55% of durene into a crystallizer, introducing small nitrogen bubbles with the flow rate of 60L/h from bottom to top, firstly cooling to-10 ℃, then cooling to-30 ℃ at the speed of 1 ℃/min, carrying out crystallization treatment for 90min, introducing small nitrogen bubbles with the flow rate of 50L/h from top to bottom, and filtering crystals deposited by crystallization for 50min through a flat porous sieve attached with nano-scale metal particles, wherein the pore diameter of the porous sieve is 3-5mm, thus obtaining a durene crude product.
(2) Heating and melting the durene crude product at 135 ℃, introducing small nitrogen bubbles with the flow rate of 45L/h from bottom to top, heating to 190 ℃ at the speed of 10 ℃/min, then continuously heating to 198 ℃ at the speed of 0.5 ℃/min, carrying out heat preservation treatment, condensing and recovering steam, and obtaining the separated and purified durene.
Comparative example 2:
(1) adding a material containing 55% of durene into a crystallizer, introducing small nitrogen bubbles with the flow rate of 60L/h from bottom to top, cooling to-10 ℃, then cooling to-30 ℃ at the speed of 1 ℃/min, carrying out crystallization treatment for 90min, filtering crystals deposited by crystallization for 50min through a flat porous sieve attached with nano-scale metal particles at the temperature of 60 ℃, wherein the pore diameter of the porous sieve is 3-5mm, and obtaining a durene crude product.
(2) Heating and melting the durene crude product at 135 ℃, introducing small nitrogen bubbles with the flow rate of 45L/h from bottom to top, heating to 190 ℃ at the speed of 10 ℃/min, then continuously heating to 198 ℃ at the speed of 0.5 ℃/min, carrying out heat preservation treatment, condensing and recovering steam, and obtaining the separated and purified durene.
The results of examining the purity and yield of durene prepared in examples 1 to 7 and comparative examples 1 to 2 are shown below:
as can be seen from the above table, the durene separation and purification method based on bubble fractional crystallization and distillation prepared by the invention has high purity and good yield.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A durene separation and purification method based on bubble fractional crystallization and distillation is characterized in that: the method comprises the following steps:
(1) adding a material containing durene into a crystallizer, introducing small nitrogen bubbles from bottom to top, cooling to-10 to-15 ℃, then cooling to-25 to-30 ℃ at the speed of 0.5-1 ℃/min, carrying out crystallization treatment, introducing the small nitrogen bubbles from top to bottom, filtering crystals settled by crystallization through an inclined porous sieve at the temperature of 56-60 ℃, and treating for 5-50min to obtain a durene crude product;
(2) heating and melting the durene crude product prepared in the step (1), introducing small nitrogen bubbles from bottom to top, heating to 190 ℃ at the speed of 5-10 ℃/min, continuing heating to 196 ℃ at the speed of 0.1-0.5 ℃/min, keeping the temperature at 198 ℃, condensing and recovering steam, and obtaining the separated and purified durene.
2. The durene separation and purification method based on gas bubble fractional crystallization and distillation as claimed in claim 1, characterized in that: in the step (1), the content of durene in the durene-containing material is not less than 45%.
3. The durene separation and purification method based on gas bubble fractional crystallization and distillation as claimed in claim 1, characterized in that: in the step (1), the gas velocity of the small nitrogen bubbles introduced from bottom to top is 40-60L/h.
4. The durene separation and purification method based on gas bubble fractional crystallization and distillation as claimed in claim 1, characterized in that: in the step (1), the time of crystallization treatment is 50-90 min.
5. The durene separation and purification method based on gas bubble fractional crystallization and distillation as claimed in claim 1, characterized in that: in the step (1), the gas velocity of the small nitrogen bubbles introduced from top to bottom is 30-50L/h.
6. The durene separation and purification method based on gas bubble fractional crystallization and distillation as claimed in claim 1, characterized in that: in the step (1), nanoscale metal particles are attached to the porous sieve.
7. The durene separation and purification method based on gas bubble fractional crystallization and distillation as claimed in claim 1, characterized in that: in the step (1), the inclination angle of the inclined porous sieve is 45-50 degrees, and the aperture of the porous sieve is 0.5-5 mm.
8. The durene separation and purification method based on gas bubble fractional crystallization and distillation as claimed in claim 1, characterized in that: in the step (2), the heating and melting temperature is 130-135 ℃.
9. The durene separation and purification method based on gas bubble fractional crystallization and distillation as claimed in claim 1, characterized in that: in the step (2), the gas velocity of the small nitrogen bubbles introduced from bottom to top is 15-45L/h.
10. The durene separation and purification method based on gas bubble fractional crystallization and distillation as claimed in claim 1, characterized in that: in the step (2), the purity of the durene separated and purified is 99.7-99.8%, and the yield is 95-98%.
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| CN110655489A (en) * | 2019-11-11 | 2020-01-07 | 安徽瑞邦生物科技有限公司 | Method for purifying 4-cyanopyridine by volatilization and recrystallization |
| CN113754530B (en) * | 2020-06-02 | 2023-09-29 | 中国石油化工股份有限公司 | Method for purifying adipic acid |
| CN111960912A (en) * | 2020-08-18 | 2020-11-20 | 连云港鹏辰特种新材料有限公司 | Method for preparing 2-methylnaphthalene by separating methylnaphthalene enrichment solution |
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